CN108440678B - Preparation method of amylose-fatty acid compound with different molecular weights - Google Patents
Preparation method of amylose-fatty acid compound with different molecular weights Download PDFInfo
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Abstract
The invention discloses a preparation method of amylose-fatty acid compounds with different molecular weights, belonging to the field of preparation of biodegradable materials. According to the invention, the amylose-fatty acid compound with different molecular weights is prepared by compounding the high molecular weight amylose and the fatty acids with different carbon chain lengths in water, organic solvents, enzymes or acid-base are not required, the preparation method is green and environment-friendly, and the application of the amylose-fatty acid compound in starch food and non-food industries is facilitated.
Description
Technical Field
The invention belongs to the field of preparation of biodegradable materials, and particularly relates to a preparation method of amylose-fatty acid compounds with different molecular weights.
Background
Amylose is a linear polysaccharide formed by connecting D-glucopyranose units through α -1, 4 glycosidic linkages, accounts for 20-30% of starch particles, can form a complex with various guest molecules including alcohols, polymers, iodine, fatty acids and the like through hydrophobic interactions, and is widely applied to food processing, starch-based biodegradable materials and responsive polymers.
The current common methods for preparing amylose-fatty acid complexes are mainly to grow the precipitated complexes in dimethyl sulfoxide (DMSO) -water mixtures or in acidic-alkaline solutions. DMSO or alkaline conditions cause solubilization of amylose, addition of fatty acids induces precipitation to form crystals of amylose complexes, which are separated by centrifugation and filtration to give amylose complexes. Lianxi Jun (Chinese patent CN201110120286.3) discloses a method for preparing amylose with a narrow molecular weight distribution range, which comprises the steps of carrying out enzymolysis on retrogradation resistant starch by using high-temperature amylase, dissolving the retrogradation resistant starch by using alkali liquor with the concentration of 2-4mol/L, and precipitating and separating the amylose by using n-butyl alcohol; gaoquyu et al (Chinese patent CN201710644842.4) discloses a method for preparing low amylose starch nanocrystals by enzymatic pretreatment in cooperation with an acid method.
However, there are a number of problems with the current methods. First, residual DMSO organic solvent in the purified complex interferes with experimental results, and the use of DMSO in the preparation process limits the use of the complex in food processing. Secondly, the use of alkaline and acidic solutions will lead to hydrolysis of amylose, and these processes for preparing amylose-fatty acid complexes are more complicated.
Therefore, the method for preparing amylose and amylose compound without using organic solvent or acid-base condition is simple, efficient and environment-friendly and receives more and more attention. The preparation of amylose and its compounds with controllable molecular weight is also one of the research hotspots in the fields of food processing and biodegradable materials nowadays.
Disclosure of Invention
Aiming at the technical problems, the invention provides a simple, high-efficiency and environment-friendly method for preparing amylose-fatty acid compounds with different molecular weights, which comprises the following specific preparation steps:
(1) weighing 1g of amylose, adding the amylose into deionized water, preparing an amylose suspension with the mass fraction of 5%, adding the amylose suspension into a polytetrafluoroethylene reaction kettle, adding 0.2g of fatty acid, mixing, sealing, placing the sealed reaction kettle into a ventilation oven, and vibrating and mixing for 1 hour at 85 ℃;
(2) after vibration mixing, heating the suspension in the reaction kettle to 160 ℃, stopping heating, then stirring the suspension, cooling to 100 ℃, placing the reaction kettle filled with the suspension in a ventilation oven after cooling, keeping the temperature and rotating for 24 hours at 85 ℃, and discharging after rotating to obtain an amylose-fatty acid compound;
(3) diluting the amylose-fatty acid compound with water at 85 ℃ until the mass fraction is 1%, centrifuging, removing supernatant, collecting precipitate, washing with hot water at 65-80 ℃ for 2-3 times, and freeze-drying to obtain white amylose-fatty acid compound powder.
The weight average molecular weight Mw of the amylose in the step (1) is 200000.
The fatty acid in the step (1) is any one of caprylic acid (C8), capric acid (C10), lauric acid (C12), myristic acid (C14) and palmitic acid (C16).
The centrifugal separation rotating speed in the step (3) is 2000rpm, and the centrifugal time is 5 minutes.
The amylose and the fatty acid with different carbon chain lengths are compounded, so that the molecular weight of the prepared amylose-fatty acid compound is controllable, and the weight average molecular weight Mw of the compound is 39000-190000.
The present invention prepares a series of amylose-fatty acid complexes by simply mixing various fatty acids (C8, C10, C12, C14, C16) and amylose (Mw of 200000) in a hot aqueous solution without enzymes, acid-base conditions and complicated routes through the above-mentioned steps, followed by simple separation and purification steps. The principle of the method is as follows:
first, vibratory mixing of the tetrafluoroethylene reactor at 85 ℃ was used to obtain a better mixture of fatty acids and amylose. Because the melting point range of fatty acids of different chain lengths is-7.9 ℃ to 63.1 ℃, the fatty acids will be totally dissolved by vibrating at 85 ℃;
second, the mixture was heated to 160 ℃ in a tetrafluoroethylene reactor at which temperature all amylose was dissolved, which facilitated the incorporation of fatty acid chains into the hydrophobic cavities of the amylose chains. Due to the different lengths of the fatty acid chains, amylose-fatty acid C8, amylose-fatty acid C10, amylose-fatty acid C14 and amylose-fatty acid C16 complexes are prepared respectively, and the lengths of the helical chain sections of the complexes are 2.02, 2.52, 3.53 and 4.02nm respectively. The invention selects amylose (M) with the same high molecular weightw200000) and the amylose fraction has polydispersity and includes amylose fractions of different molecular weights (lengths)The complex can be matched and complexed with fatty acids C8, C10, C14 and C16 with different lengths to form a complex, the molecular weight of the complex is 39000-190000 as the length of the fatty acid is increased from C8 to C16;
third, the amylose-fatty acid complex initially obtained was slowly cooled to 100 ℃, and then the complex was rotated at 85 ℃ for 24 hours, which allowed the formation and precipitation of a crystalline complex. Since this temperature (85 ℃) is above the onset temperature of amylose retrogradation and above the melting point of the fatty acids, both the uncomplexed amylose and the fatty acids remain in solution. Diluting the suspension of amylose-fatty acid complex with water at 85 deg.C to a mass fraction of 1%, centrifuging, discarding the supernatant containing non-complex fatty acid and amylose, collecting the precipitate, washing twice with hot water, and finally freeze-drying to obtain white powder of amylose-fatty acid complex.
The invention has the beneficial effects that:
(1) in the traditional method for preparing the amylose-fatty acid compound, the amylose with lower molecular weight is obtained by catalyzing the degradation of the amylose by enzyme or acid and alkali, and then the amylose and the fatty acid are subjected to compound precipitation through a series of preparation steps, so that the preparation route is longer and more complex, and biological agents such as protease and the like are expensive; the invention does not need acid-base conditions and complex routes, and only simply mixes various fatty acids and amylose in hot water solution to prepare a series of amylose-fatty acid compounds;
(2) the invention selects the amylose with the same high molecular weight, simply regulates and controls the fatty acid with different carbon chain lengths to obtain the amylose-fatty acid compound with different molecular weights, takes water as a solvent, avoids the residue of organic solvents and other chemical reagents, and is beneficial to the application of the amylose-fatty acid compound in the food processing industry.
Detailed Description
The invention is described in more detail below with reference to the following examples:
examples 1 to 5 were conducted by complexing caprylic acid (C8), capric acid (C10), lauric acid (C12), myristic acid (C14), palmitic acid (C16) and amylose to prepare complexes, and testing the molecular weight and distribution of the complexes.
Example 1
(1) Weighing 1g of amylose (Mw is 200000), adding into deionized water, preparing amylose suspension with mass fraction of 5%, adding into a polytetrafluoroethylene reaction kettle, adding 0.2g of octanoic acid (C8), mixing, sealing, placing the sealed reaction kettle into a ventilation oven, and mixing under vibration at 85 deg.C for 1 hr;
(2) after vibration mixing, heating the suspension in the reaction kettle to 160 ℃, stopping heating, then stirring the suspension, cooling to 100 ℃, placing the reaction kettle filled with the suspension in a ventilation oven after cooling, and keeping the temperature and rotating for 24 hours at 85 ℃ to obtain an amylose-fatty acid compound;
(3) diluting the amylose-fatty acid compound with water at 85 ℃ to 1 mass percent, centrifuging at 2000rpm for 5 minutes, discarding the supernatant, collecting the precipitate, washing with 65 ℃ hot water for 2 times, and freeze-drying to obtain white amylose-fatty acid compound powder.
Example 2
(1) Weighing 1g of amylose (Mw is 200000), adding into deionized water, preparing amylose suspension with mass fraction of 5%, adding into a polytetrafluoroethylene reaction kettle, adding 0.2g of capric acid (C10), mixing, sealing, placing the sealed reaction kettle into a ventilated oven, and mixing under vibration at 85 deg.C for 1 hr;
(2) after vibration mixing, heating the suspension in the reaction kettle to 160 ℃, stopping heating, then stirring the suspension, cooling to 100 ℃, placing the reaction kettle filled with the suspension in a ventilation oven after cooling, and keeping the temperature and rotating for 24 hours at 85 ℃ to obtain an amylose-fatty acid compound;
(3) diluting the amylose-fatty acid compound with water at 85 ℃ to 1 mass percent, centrifuging at 2000rpm for 5 minutes, discarding the supernatant, collecting the precipitate, washing with hot water at 70 ℃ for 2 times, and freeze-drying to obtain white amylose-fatty acid compound powder.
Example 3
(1) Weighing 1g of amylose (Mw is 200000), adding into deionized water, preparing amylose suspension with mass fraction of 5%, adding into a polytetrafluoroethylene reaction kettle, adding 0.2g of lauric acid (C12), mixing, sealing, placing the sealed reaction kettle into a ventilated oven, and mixing under vibration at 85 deg.C for 1 hr;
(2) after vibration mixing, heating the suspension in the reaction kettle to 160 ℃, stopping heating, then stirring the suspension, cooling to 100 ℃, placing the reaction kettle filled with the suspension in a ventilation oven after cooling, and keeping the temperature and rotating for 24 hours at 85 ℃ to obtain an amylose-fatty acid compound;
(3) diluting the amylose-fatty acid compound with water at 85 ℃ to 1 mass percent, centrifuging at 2000rpm for 5 minutes, discarding the supernatant, collecting the precipitate, washing with hot water at 70 ℃ for 2 times, and freeze-drying to obtain white amylose-fatty acid compound powder.
Example 4
(1) Weighing 1g of amylose (Mw is 200000), adding into deionized water, preparing amylose suspension with mass fraction of 5%, adding into a polytetrafluoroethylene reaction kettle, adding 0.2g of myristic acid (C14), mixing, sealing, placing the sealed reaction kettle into a ventilated oven, and mixing under vibration at 85 deg.C for 1 hr;
(2) after vibration mixing, heating the suspension in the reaction kettle to 160 ℃, stopping heating, then stirring the suspension, cooling to 100 ℃, placing the reaction kettle filled with the suspension in a ventilation oven after cooling, and keeping the temperature and rotating for 24 hours at 85 ℃ to obtain an amylose-fatty acid compound;
(3) diluting the amylose-fatty acid compound with water at 85 ℃ to 1 mass percent, centrifuging at 2000rpm for 5 minutes, discarding the supernatant, collecting the precipitate, washing with hot water at 75 ℃ for 2 times, and freeze-drying to obtain white amylose-fatty acid compound powder.
Example 5
(1) Weighing 1g of amylose (Mw is 200000), adding into deionized water, preparing amylose suspension with mass fraction of 5%, adding into a polytetrafluoroethylene reaction kettle, adding 0.2g of palmitic acid (C16), mixing, sealing, placing the sealed reaction kettle into a ventilated oven, and mixing under vibration at 85 deg.C for 1 hr;
(2) after vibration mixing, heating the suspension in the reaction kettle to 160 ℃, stopping heating, then stirring the suspension, cooling to 100 ℃, placing the reaction kettle filled with the suspension in a ventilation oven after cooling, and keeping the temperature and rotating for 24 hours at 85 ℃ to obtain an amylose-fatty acid compound;
(3) diluting the amylose-fatty acid compound with water at 85 ℃ to 1 mass percent, centrifuging at 2000rpm for 5 minutes, discarding the supernatant, collecting the precipitate, washing with hot water at 80 ℃ for 3 times, and freeze-drying to obtain white amylose-fatty acid compound powder.
The results of the amylose-fatty acid tests prepared in examples 1, 2 and 4 are shown in table 1:
TABLE 1 molecular weight test results for amylose-fatty acids
Claims (3)
1. A preparation method of amylose-fatty acid compounds with different molecular weights is characterized by comprising the following preparation steps:
(1) weighing 1g of amylose with the weight-average molecular weight Mw of 200000, adding the amylose into deionized water, preparing amylose suspension with the mass fraction of 5%, adding the amylose suspension into a polytetrafluoroethylene reaction kettle, adding 0.2g of fatty acid, mixing, sealing, placing the sealed reaction kettle into a ventilation oven, and vibrating and mixing for 1 hour at 85 ℃; the fatty acid is any one of caprylic acid, capric acid, lauric acid, myristic acid and palmitic acid;
(2) heating the suspension in the reaction kettle to 160 ℃ after vibration mixing, then stirring the suspension to cool to 100 ℃, placing the reaction kettle filled with the suspension in a ventilation oven after cooling, preserving heat and rotating for 24 hours at 85 ℃, discharging after rotating, and obtaining an amylose-fatty acid compound;
(3) diluting the amylose-fatty acid compound with water at 85 ℃ until the mass fraction is 1%, centrifuging, removing supernatant, collecting precipitate, washing with hot water at 65-80 ℃ for 2-3 times, and freeze-drying to obtain white amylose-fatty acid compound powder.
2. The method of claim 1, wherein the amylose-fatty acid complex of different molecular weights is prepared by: the centrifugal separation rotating speed in the step (3) is 2000rpm, and the centrifugal time is 5 minutes.
3. The method of claim 1, wherein the amylose-fatty acid complex of different molecular weights is prepared by: the weight average molecular weight Mw of the amylose-fatty acid compound in the step (3) is 39000-190000.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914163A (en) * | 2010-08-26 | 2010-12-15 | 华南理工大学 | Chronic digestible starch and preparation method thereof |
| CN103288972A (en) * | 2013-06-28 | 2013-09-11 | 山东农业大学 | Method for producing stearic acid starch ester through homogeneous dry process |
| CN104961837A (en) * | 2015-06-30 | 2015-10-07 | 华南理工大学 | Preparation method of starch and fatty acid compound |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914163A (en) * | 2010-08-26 | 2010-12-15 | 华南理工大学 | Chronic digestible starch and preparation method thereof |
| CN103288972A (en) * | 2013-06-28 | 2013-09-11 | 山东农业大学 | Method for producing stearic acid starch ester through homogeneous dry process |
| CN104961837A (en) * | 2015-06-30 | 2015-10-07 | 华南理工大学 | Preparation method of starch and fatty acid compound |
Non-Patent Citations (1)
| Title |
|---|
| Effect of fatty acids on the rheological behaviour of amylomaize;Stylianos N. Raphaelides et al.;《Food Research International》;20071018;第44卷(第1期);第75-78页 * |
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